Thermochimica Acta 671 (2019) 83–88
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Thermochimica Acta
journal homepage: www.elsevier.com/locate/tca
Experimental investigation on thermal properties of Ag nanowire nanofluids
at low concentrations
T
R. Carbajal-Valdéza, A. Rodríguez-Juárezb, J.L. Jiménez-Pérezb, , J.F. Sánchez-Ramírezc,
A. Cruz-Oread, Z.N. Correa-Pachecoe, M. Maciasd, J.L. Luna-Sánchezb
⁎
a
CONACYT, SENER-Instituto Tecnológico de Celaya, Antonio García Cubas 600. Col. Fovissste, Celaya, Guanajuato, Mexico
UPIITA-Instituto Politécnico Nacional, Avenida Instituto Politécnico Nacional No. 2580, Col Barrio la Laguna Ticomán, Gustavo A. Madero, Ciudad de México, C.P.
07340, Mexico
c
Instituto Politécnico Nacional-CIBA, Ex-Hacienda San Juan Molino Carretera Estatal Tecuexcomac-Tepetitla Km 1.5, Tlaxcala, C.P. 90700, Mexico
d
Departamento de Física, Centro de Investigación y de Estudios Avanzados del Instituto Politécnico Nacional-IPN, Av. IPN No. 2508, Col. San Pedro Zacatenco, 07360,
Ciudad de México, Mexico
e
CONACYT, Centro de Desarrollo de Productos Bióticos-Instituto Politécnico Nacional (CEPROBI-IPN), Carretera Yautepec-Jojutla, Km. 6, calle CEPROBI No. 8, Col. San
Isidro, Yautepec, Morelos, C.P. 62731, Mexico
b
A R TICL E INFO
A BSTR A CT
Keywords:
Nanowires
Photothermal techniques
Thermal parameters
Nanofluids
tHermal conductivity
New nanofluids containing Ag nanowires with different concentrations were prepared by chemical reduction
method. The metallic nanowires were monodispersed and soluble in distilled water. Thermal properties of nanofluids containing Ag nanowires were obtained using photothermal techniques. The thermal-wave resonator
cavity (TWRC) technique was used to obtain the samples’ thermal diffusivity. Open Photoacoustic Cell (OPC)
technique was used to obtain the thermal effusivity of Ag nanowires. The thermal diffusivity and effusivity were
obtained by fitting the theoretical expressions for each configuration as a function of the sample thickness and
frequency to the experimental data. The thermal properties of the nanofluids seems to be strongly dependent of
Ag nanowire concentration. It was observed an increase of thermal parameters when concentration of nanowires
increased. Thermal conductivity behavior of the nanofluids is explained. UV–vis spectroscopy, Scanning Electron
Microscopy (SEM), Energy-dispersive X-ray spectroscopy (EDS) and X-ray diffraction (XRD) techniques were
used to characterize the nanofluids.
1. Introduction
In recent years, nanofluids have attracted great interest in the industry and in the scientific community. The most important applications of nanofluids are in heat transport and its thermophysical properties such as thermal conductivity, viscosity and dielectric constant
have been enhanced by the use different concentrations of nanoparticles, nanowires or nanotubes [1]. However, the thermal efficiency
of natural fluids is not enough effective and can cause damage to machines where a cooling system is required, resulting in overheating.
This increase causes the thermal conductivity of the industrial fluids to
increase, hence, the fluids are in the spotlight in day-to-day industrial
work. Current research has found that the addition of nanoparticles in
fluids can improve the efficiency of the thermal properties of the fluid,
such as conductivity, diffusivity and thermal effusivity. An example of
this, is the work of Choi et al. [2]. They found that the thermal conductivity was improved by 160% by adding 1% of carbon nanotubes
⁎
volumetric fraction in an oil suspension. According to other investigations, different materials, sizes, shapes and concentrations of nanoparticles were used to improve the thermal conductivity of nanofluids
[1–5]. Among particles, metal nanoparticles have deserved special attention because of surface electron oscillations caused by the surface
plasmon resonance (SPR) effect. Of special importance are the silver
nanoparticles (Ag) because they have low production cost and are easily available, being used for shape-controlled synthesis [1,6–7]. They
have been often used as thermal additives for preparation of nanofluids
[8,9]. In many works, spherical silver nanoparticles have been studied,
however, the effect of low concentrations has been rarely considered
[10–13]. Nanostructures such as nanowires have been used in nanofluids, due to the surface-volume ratio that increases the heat transfer
[14]. It is important to highlight that there are few researchers who
have added nanowires in fluids in small proportions in order to enrich
this fluid from the point of view of Nanotechnology. On the other hand,
the evaluation on the thermal conductivity of nanofluids has not been
Corresponding author.
E-mail address: jimenezp@fis.cinvestav.mx (J.L. Jiménez-Pérez).
https://doi.org/10.1016/j.tca.2018.11.015
Received 11 July 2018; Received in revised form 23 September 2018; Accepted 18 November 2018
Available online 19 November 2018
0040-6031/ © 2018 Elsevier B.V. All rights reserved.
Thermochimica Acta 671 (2019) 83–88
R. Carbajal-Valdéz et al.
accomplished. In this work, silver nanowires were added in distilled
water at low concentrations to study their thermophysical properties by
thermal-wave resonator cavity (TWRC) and open cell photoacoustic
(OPC) techniques with the purpose of producing more effective, stable
and uniform nanofluids. It was found, that the heat transfer of the fluid
was improved, therefore Ag nanowire-based nanofluids could have
possible applications in heat transport to reduce the losses of heat
transfer in industrial machines of high efficiency, in the field of cooling
of electronic equipment, in solar energy systems, heat exchangers and
machining processes.
2.3. Open photoacoustic cell (OPC)
OPC technique, was used for the thermal effusivity measurements
[17]. In this technique, a laser beam is modulated by using a mechanical chopper, at an angular frequency ω = 2πf. The details of the
cross section of the photoacoustic cell and experimental cell are shown
in Figs. 2 and 3. In the OPC technique, the liquid sample is placed on an
aluminum foil, of known thermal effusivity. An electret microphone
connected to the cell detects the heat generated due to the temperature
rise and then it diffuses into the photoacoustic (PA) gas chamber
modulating the pressure (acoustic waves) within the PA cell. A lock-in
amplifier interfaced with a data acquisition system measures the microphone-response signal.
For the calculation of the thermal effusivity the obtained photoacoustic signal of each sample is normalized, by using the photoacoustic signal when the sample is air, and the following equation was
used [18]:
2. Theory
Thermal diffusivity and effusivity of the nanofluids were measured
by using the TWRC and OPC techniques [15–18].
2.1. Thermal wave resonator cavity (TWRC)
es =
l0
0 c0
IR
(2)
In this work different concentrations of nanoliquids were acquired
and their thermal diffusivities measured by a cavity-length scan in the
TWRC device.
The temperature fluctuations at x = l, interface between sample and
pyroelectric (PE) detector, can be detected with the PE sensor as a
function of the sample thickness. The PPE (photopyroelectric) signal is
amplified by the lock-in amplifier, at the reference of the beam modulation frequency (f), where its PPE amplitude and phase are measured
as a function of the sample thickness (l).
For the situation in which the sample in the TWRC may be considered as thermally thick, i.e., |ql| > 1, where q = (2π f i/Ds)1/2, with i
= (−1) ½ and Ds the sample thermal diffusivity,
the PE sensor output voltage, is given by Eq. (1) [15,16].
where 0 is the density of the used aluminum foil (2.7 gcm−3), c0 is the
specific heat of the aluminum foil (0.9 Jg-1 °C-1), l 0 is the thickness of
the aluminum foil (16 μm), = 2 f being f the modulation frequency
of the excitation beam in the sample, and IR is the slope of the normalized photoacoustic signal, as a function of the square root of f. The
cell was calibrated with water in order to compare with the values
reported in the literature. The obtained value for distilled water was
(e H2 O = 1487.05 ± 47 Ws1/2 / m2°C ) and the reported value is
e H2 O = 1570 Ws1/2 / m2°C [19]). It can be seen that the obtained value
was similar to the reported one.
V (l) = V0exp(−ql)
2.4. Materials
(1)
where V0 is a modulation frequency-dependent factor.
Eq. (1) is a complex equation because q is a complex quantity,
contains the factor i = (−1) ½, then this equation can be represented in
polar coordinates, which have a module, related directly with the experimental amplitude data measured by the lock-in amplifier, and a
phase, related directly with the experimental phase data measured by
the same lock-in amplifier.
Since the PE signal, for thermally thick samples, depends on the
sample thickness (ls) in a simple linear way, as is shown in Eq. (1), the
thermal diffusivity can be obtained from the slope of the natural
logarithm of the PPE signal amplitude or from the slope of the PPE
signal phase, as a function of l.
For silver nanowires synthesis, the following reactants without
treatment were used: silver nitrate (AgNO3 99.6%, Aldrich), PVP (PM
55,000 g/mol, Aldrich), glycerol (C3H5(OH)3, 99.90%, J.T. Baker) and
sodium chloride (NaCl, 99.0%, Meyer).
2.5. Preparation of silver nanowires (AgNWs)
The procedure adopted for AgNWs synthesis was as follows: 0.6 g of
PVP were dissolved with 19 mL of glycerol during 36 h at room temperature. Then, the solution was added into a round-bottom flask and
0.158 g of AgNO3 were added to the solution with vigorous stirring until
AgNO3 was fully dissolved. Afterwards, a solution of 5.85 mg of NaCl in
0.05 mL of H2O was prepared and 1 mL of glycerol was added. The last
solution was put into the flask and the reaction temperature of the
mixture rapidly raised to 220 °C (roughly with a heating speed of
2.75 °C/min) on a hot plate (Cornic model PC-4200) with magnetic
stirring at 50 rpm in aerated condition. When the reaction was stopped
and the flask cooled down to room temperature, deionized water was
added into the flask in a 1:1 vol ratio, and then the mixture was centrifuged at 7000 rpm until all visible products were collected. The
transparent supernatant was discarded and the obtained AgNWs were
washed with water three times to remove the PVP residue.
Then, the nanowires were dispersed in ethanol and again centrifuged at 4000 rpm for 10 min. The final product was dispersed in
distilled water to obtain nanofluids containing AgNWs with different
concentrations and the thermal measurement and further characterization were done. The obtained dispersion did not contain any visible
solids and was stable for more than three months without significant
changes in the spectral pattern indicating that these nanofluids are
highly stable (see Fig. 4).
2.2. TWRC experimental setup
In the TWRC technique, a cavity consists of two parallel walls: one
wall acts as the thermal-wave generator and the other wall is a pyroelectric transducer as shown in Fig. 1. The experimental arrangement
consists of a diode laser whose beam was modulated by the internal
oscillator of a lock-in amplifier at 4 Hz. The modulated light impinges
on a thin copper foil of 100 μm thick mounted on an automatic cylindrical micrometer stage controlled by a PC. This stage allowed the
cavity length to vary with a 1 μm step resolution. The modulated light
was absorbed on the highly conducting thin copper foil, which acted as
an optical-to-thermal power converter. The cylindrical module was
dipped in the sample as showed in Fig. 1. Thermal waves conducted
across the liquid interface reached the PVDF pyroelectric sensor of
110 μm thickness. The PE signal generated in the sensor was amplified
by a lock-in amplifier. The complex Eq. 1 was adjusted in the amplitude
and phase to the experimental amplitude and phase data, as mentioned
before. All measurements were performed at room temperature.
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R. Carbajal-Valdéz et al.
Fig. 1. Thermal-wave resonant cavity (TWRC) experimental set-up.
Fig. 2. Open photoacoustic cell (OPC) experimental setup.
Fig. 4. UV–vis absorption spectra of nanowires nanofluids obtained (̶) immediately after preparation and (—) after three months.
path length of 1 cm. The nanofluid was place in a quartz cell. Powder Xray diffraction (XRD) spectra of the AgNWs were obtained using a
PANalytical X-ray Diffractometer, Model X’pert, with a CuKα radiation
(λ = 1.transm5406 Å), 40 kV– 40 mA, 2θ/θ scanning mode. Data was
taken for the 2θ range of 30 to 90 ° with a step of 0.02 and speed of 2 s/
step.
3. Results and discussion
Silver nanowires were synthesized by polyol process. The polyol
process is based on reduction of an inorganic salt by a polyol at an
elevated temperature. A polyol is a compound with multiple hydroxyl
functional groups available for organic reactions. In the polyol method,
glycerol is used as both, solvent and reducing agent, PVP is used as
stabilizing agent, and AgNO3 is used as Ag source.
The UV–vis absorption spectrum of the synthesized solution is
shown in Fig. 4. The plasmon absorption peak appeared at 378 nm as
indicative of AgNWs formation. A shoulder peak appeared at about
350 nm and is an optical characteristic for bulk silver. Absence of absorption peak at wavelengths higher than 400 nm indicates that the
final product is thoroughly AgNWs [17]. Nevertheless, the wide peak
may indicate that a small amount of other morphologies such as
spherical nanoparticles are present.
Fig. 3. Cross section of the open photoacoustic cell (OPC).
2.6. Characterization
The AgNWs morphology was analyzed by Scanning electron microscopy (Vega©tescan SN: VG1540475MX) at 15 kV. UV–vis analysis
was performed on a GENESYS 10S UV–vis Spectrophotometer GD10S
UV–vis from 300 to 600 nm with a slit wavelength of 2 nm and light
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Fig. 5. AgNWs morphology: (a) SEM image of AgNWs (magnification 2750) and (b) normalized diameter size distribution of AgNWs; average diameter was calculated from Gaussian fitting of the histogram.
SEM images of the synthesized AgNWs is shown in Fig. 5. From the
images, it can be observed that the AgNWs are very homogenous in
morphology. It is clearly shown that AgNWs with a length up to 10 μm
have been synthesized with high yield. The diameter of the nanowires
was 96.04 nm with a standard deviation of 13.67%, indicating that the
AgNWs are homogenous.
Fig. 6 shows the typical XRD pattern of AgNWs. The diffraction
peaks occurring at 38.1°, 44.82°, 64.62°, 77.2°, and 81.56° are indexed
as (111), (200), (220), (311), and (222) facets, being consistent well
with a face-centered-cubic (fcc) Ag crystalline structure which is in
accordance with the literature presented by Yang et al. 2015 [20]
(JCPDS card number 87-0717).
The calculated lattice constants according to the spacing distance dg
of the {111} planes and the equation: 1/ d2 = h2 + k2 + l2/a2 is 4.088 Å
[21] and it is in agreement with the literature value of 4.086 Å. No
peaks for other crystal types are observed. The sharp diffraction peaks
indicated the sample having a high crystallinity. Therefore, pure silver
nanowires were obtained under the present synthesis conditions. The
intensity ratios of (111)/(200) and (111)/(220) peaks were 5.58 and
7.59 respectively, which were relatively higher than the conventional
2.5 and 4 values which are described by Li et al. [22]. Therefore, this
would indicate that the {111} planes of silver tend to be preferentially
oriented for the polyol method.
The PE signal amplitude is shown in Fig. 7, as a function of the
cavity length from the AgNWs sample in the TWRC experiment. The
solid line, represents the best linear fit of Eq. (1) to the experimental PE
data of the ln(amplitude). From this fit, the obtained mean thermal
diffusivity was (16.04 ± 0.17) × 10−8 m2 s−1 for the sample with
concentration of 7 × 10−4 Vol. %. Similar measurements were carried
out to determine the thermal diffusivity for the other concentrations.
Resulting thermal-diffusivity values of the AgNWs are summarized in
Table 1.
Fig. 8 shows the typical behavior of the normalized OPC signal, as a
Fig. 7. Natural logarithm of the TWRC signal amplitude as a function of the
relative cavity length for AgNWs with concentration of 7 × 10−4 Vol. %.
Fig. 6. XRD pattern of silver nanowires synthesized by polyol process.
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R. Carbajal-Valdéz et al.
In order to compare the obtained results with reported values in the
literature, it was found the value of thermal conductivity for water
(k = 0.613 W/m K [23]), thermal diffusivity (D = 14.0 × 10−8 m2/s
[24]) and thermal effusivity (e = 1570 W s1/2/ m2 K [19]), that are very
near with the calibration obtained values in this study.
From the results obtained in this work, it was found that the thermal
conductivity enrichment of the AgNWs (φ = 96 nm × 40 μm) was from
4 to 20.8 for volumetric fraction between 3.5 × 10−6 and 1.74 × 10-4
vol. %., as shown in Fig. 9. Thermal conductivity enhancement increase
in a non-linear way for low volume concentrations. Similar results were
reported for Ag spherical nanoparticles with 55 nm in size, with concentrations from 1 × 10-5 to 1.02 × 10-3 vol. % and thermal conductivity enhancement from 4 to 21.0 Vol. %, respectively and also
with increase non-linear way for low Vol % [25]. The high thermal
conductivity enhancement of the AgNWs, can be related with the specific surface area of the nanowires compared with Ag spherical nanoparticles, layering at the liquid solid surface interface and also Brownian motion may be responsible for enhancement. However, our results
are in good agreement with many research works [25,26] i.e., the
thermal conductivities of nanofluids increase as particle volume concentration increase.
It is interesting to note that the model by Patel et al. [26] quite
accurately match with the experimental data for silver-water nanofluids
which show a non-linear increase of thermal conductivity as a function
of concentration.
From the comparisons, due to there are few works related to
thermal conductivity of AgNWs at low concentrations to compare with
our experimental results, it is concluded, that further research is needed
to develop a suitable model to predict the anomalous increase of
thermal conductivity in nanofluids of which will take into account
several possible factors in enhancing the heat transfer performance of
nanofluids [25,26].
Table 1
Thermal diffusivity (D), effusivity (e), volumetric heat capacity (ρc), conductivity (k) and thermal conductivity enhancement of the evaluated samples.
AgNws/water
(Vol. %)
Diffusivity
D(10−8 m2/s)
Effusivity
e(Ws1/2/m2K)
Conductivity
Knf (W/mK)
Conductivity
enhancement
((knf – kbf) /
kbf)×100(%)
3.5 × 10−6
4.7 × 10−6
7.0 × 10−4
1.36 × 10−4
1.74 × 10−4
14.00
15.11
16.04
16.58
17.75
1663
1687
1688
1694
1716
0.622
0.656
0.676
0.690
0.723
4
9.6
13
15.2
20.8
±
±
±
±
±
0.18
0.20
0.17
0.16
0.24
±
±
±
±
±
32
26
41
125
52
±
±
±
±
±
0.013
0.011
0.017
0.051
0.023
where kbf = kwater = 0.61 W/ m K.
Fig. 8. OPC signal, as a function of the f1/2(s−1/2) for Ag NWs with concentration of 7 × 10-4 Vol. %.
4. Conclusions
In summary, silver nanowires (AgNWs) were successfully prepared
using the polyol process. Subsequently, the physicochemical properties
of AgNWs were investigated by UV–vis spectroscopy, SEM and XRD.
Also, a complete thermal characterization of AgNWs was achieved by
using two different photothermal techniques. Thermal diffusivity and
thermal effusivity of the nanofluids were obtained at room temperature
using the TWRC and OPC, respectively. The thermal conductivity (k)
values were calculated from the definition of the thermal diffusivity (D
= k/ (ρc)) and thermal effusivity e = (kρc)1/2. AgNWs showed an effective thermal transport property for low concentrations, as seen experimentally. For 3.5 × 10−6 vol% of AgNWs in the fluid, and enhancement of 4% was achieved, while an enhancement of 20.8% in
thermal conductivity was found for 1.74 × 10-4 volume fraction of
AgNWs. However, more research and new thermal models are necessary to predict the thermal properties of nanofluids. This study is a
promising way for the elaboration of nanowires which can be used in
heat transfer applications.
Fig. 9. Ag nanofluids thermal conductivity enhancement of for different concentrations of AgNWs.
function of the f1/2(s−1/2), where f is the light modulation frequency
from the AgNWs (for the concentration sample of 7 × 10-4 vol%). The
solid lines, in Fig. 8 shows the best fit of the Eq. (2) to the normalized
OPC data. From this fit the obtained thermal effusivity for this sample is
1688.00 ± 41 Ws1/2/m2K. Similar measurements were carried out to
determine the thermal effusivity of the AgNWs for the other samples.
The values of thermal effusivity of Ag nanowires are summarized in the
Table 1. Taking into consideration the definition of the thermal diffusivity (D=k/(ρc)) and thermal effusivity (e = (k ρc)1/2), where k is the
thermal conductivity and ρc is the volumetric heat capacity, with ρ the
density and c the specific heat, it is possible to obtain the k and ρc
values from the obtained values of thermal diffusivity and thermal effusivity of the AgNWs. The values of thermal conductivity are shown in
Table 1.
Acknowledgements
Thanks to CONACYT, COFAA, CGPI-IPN, Mexico, and RedNanofotónica, for their partial financial support.
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